ZIF合成总结

序号配体条件结构来源1AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.09g,3.44×10-4mol)andimidazole(H-IM)(0.15g,2.20×10-3mol)wasdissolvedin18mLDMFina20-mLvial.Thevialwascappedandheatedfor24hina85ºCisothermaloven.Thevialwasthenremovedfromtheovenandallowedtocooltoroomtemperaturenaturally.ColorlesscubiccrystalsofZIF-1thusproducedwerewashedwithDMF(3mL×3)anddriedinair(10min)(ZIF-1crb):Zn(IM)2·(Me2NH)Doi/10.1073/pnas.06024391032(ZIF-3dft):Zn(IM)2AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.010g,3.82×10-5mol)andimidazole(H-IM)(0.030g,4.41×10-4mol)wasaddedina4-mLvialanddissolvedinamixedsolventofDMF(2mL)andNMP(1mL).Thevialwascappedandheatedfor4dina85ºCisothermaloven.Thevialwasthenremovedfromtheovenandallowedtocooltoroomtemperaturenaturally.Severalprism-shapedcrystalsformedatthebottomofthevialalongwithsomewhitepowder-likeprecipitate.ThecrystalsofZIF-3werecollectedmanuallyforsinglecrystalX-raystructuredetermination..Doi/10.1073/pnas.06024391033(ZIF-4cag):Zn(IM)2·(DMF)(H2O)AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.040g,1.53×10-4mol)andimidazole(H-IM)(0.030g,4.41×10-4mol)wasdissolvedin3mLDMFina4-mLvial.Thevialwascappedandheatedatarate5ºC/minto130ºCinaprogrammableoven,heldatthistemperaturefor48h,thencooledatarateof0.4ºC/mintoroomtemperature.ColorlessrhombohedralcrystalsofZIF-4thusproducedwerewashedwithDMF(3mL×3)anddriedintheair(10min)Doi/10.1073/pnas.06024391034(ZIF-10mer):Zn(IM)2.AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.010g,3.82×10-5mol)andimidazole(H-IM)(0.030g,4.41×10-4mol)wasdissolvedin3mLDMFina4-mLvial.Thevialwascappedandheatedfor4dinanisothermalovenat85ºC.Thereactionmixturewasthenallowedtocooltoroomtemperaturenaturally.Severalblock-shapecrystalsofZIF-10formedonthewallandbottom,andwereseparatedbyhandandcollectedforsinglecrystalX-raystructuredetermination.Doi/10.1073/pnas.06024391035(ZIF-2crb):Zn(IM)2.0.265mLimidazolestocksolution(0.150M,3.98×10-5mol)and0.035mLZn(NO3)2·4H2Ostocksolution(0.075M,2.63×10-6mol).Theproductwasintheformofsmallrod-shapedsinglecrystals.Doi/10.1073/pnas.06024391036(ZIF-6gis):Zn(IM)2.0.257mLimidazolestocksolution(0.150M,3.86×10-5mol)and0.043mLZn(NO3)2·4H2Ostocksolution(0.075M,3.23×10-6mol).Theproductwasintheformoflargeinter-grownblocks,whichcouldbecutintosmallsinglecrystalsunderanopticalmicroscope.Doi/10.1073/pnas.06024391037(ZIF-5gar):In2Zn3(IM)12Indiumnitratepentahydrate,In(NO3)3·5H2O(0.156g,4.0×10-4mol),zincnitratetetrahydrateZn(NO3)2·4H2O(0.026g,1.0×10-4mmol)andimidazole(H-IM)(0.136g,2×10-3mol)weredissolvedinamixedsolventofDEF/n-butanol(4mL/2mL,).Aftertheadditionoftetraethylammoniumhydroxide(0.05mL,35%aqueoussolution),themixturewastransferredintoaTeflon-linedParrstainlesssteelvessel(23mL)andheatedat150ºCfor72hoursunderautogenouspressure.Pale-yellowcrystalsthusproducedwerewashedwithethanolanddriedinair(yield:70%,basedonzincnitratetetrahydrate).Doi/10.1073/pnas.06024391038AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.030g,1.15×10-4mol)andbenzimidazole(H-PhIM)(0.010g,8.46×10-5mol)wasdissolvedin3mLDMFina4-mLvial.Thevialwascappedandheatedatarateof5ºC/minto130ºCinaprogrammableoven,heldatthistemperaturefor48h,thencooledatarateof0.4ºC/mintoroomtemperature.Afterremovalofmotherliquorfromthemixture,chloroform(3mL)wasaddedtothevial.ColorlesscubiccrystalsofZIF-7werecollectedfromtheupperlayer,washedwithDMF(3mL×3)anddriedinair(10min)(ZIF-7sod):Zn(PhIM)2·(H2O)3.Doi/10.1073/pnas.06024391039(ZIF-9sod):Co(PhIM)2·(DMF)(H2O)solidmixtureofcobaltnitratehexahydrateCo(NO3)2·6H2O(0.210g,7.21×10-4mol)andbenzimidazole(H-PhIM)(0.060g,5.08×10-4mol)wasdissolvedin18mLDMFina20-mLvial.Thevialwascappedandheatedatarateof5ºC/minto130ºCinaprogrammableoven,heldatthistemperaturefor48h,thencooledatarateof0.4ºC/mintoroomtemperature.PurplecubiccrystalsthusproducedwerewashedwithDMF(3mL×3)anddriedinair(10min)Doi/10.1073/pnas.060243910310AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.60g,2.3×10-3mol)andbenzimidazole(H-PhIM)(4.2g,3.5×10-2mol)wasdissolvedin360mLDEFina500-mLwide-mouthglassjar.Thecappedjarwasheatedfor4dinanisothermalovenat100ºC.Thejarwasthenremovedfromtheoven,andallowedtocooltoroomtemperaturenaturally.Cubiccolorlesscrystalsformedonthewallsofthejaralongwithacrystallinepowderatthebottom.ColorlesscrystalsofZIF-11werecollectedbyfiltration,washedwithDMF(200mL×2)anddriedintheair(30min)(ZIF-11rho)Zn(PhIM)2·(DEF)0.9Doi/10.1073/pnas.060243910311AsolidmixtureofcobaltnitratehexahydrateCo(NO3)2·6H2O(0.010g,3.44×10-5mol)andbenzimidazole(H-PhIM)(0.030g,2.54×10-4mol)wasdissolvedin3mLDEFina4-mLvial.Thecappedvialwasheatedfor2dinanisothermalovenat130ºC.Thereactionmixturewasthenallowedtocooltoroomtemperaturenaturally.SeveralcubiccrystalsofZIF-12formedatthebottomandonthewallofthevial,andtheywerecollectedforsinglecrystalX-raystructuredetermination.(ZIF-12rho):Co(PhIM)2.Doi/10.1073/pnas.060243910312AsolidmixtureofzincnitratetetrahydrateZn(NO3)2·4H2O(0.210g,8.03×10-4mol)and2-methylimidazole(H-MeIM)(0.060g,7.31×10-4mol)wasdissolvedin18mLDMFina20-mLvial.Thevialwascappedandheatedatarateof5ºC/minto140ºCin